arXiv subjects

Gerhard Dehm

Publications and source records attributed to Gerhard Dehm.

51 records · Page 3Linked to original sources

arXiv2021

Dopant-segregation to grain boundaries controls electrical conductivity of n-type NbCo(Pt)Sn half-Heusler alloy mediating thermoelectric performance

Science-driven design of future thermoelectric materials requires a deep understanding of the fundamental relationships between microstructure and transport properties. Grain boundaries in polycrystalline materials influence the thermoelectric performance through the scattering of phonons or the trapping of electrons due to space-charge effects. Yet, the current lack of careful investigations on grain boundary-associated features hinders further optimization of properties. Here, we study n-type NbCo1-xPtxSn half-Heusler alloys, which were synthesized by ball milling and spark plasma sintering (SPS). Post-SPS annealing was performed on one sample, leading to improved low-temperature electrical conductivity. The microstructure of both samples was examined by electron microscopy and atom probe tomography. The grain size increases from ~230 nm to ~2.38 μm upon annealing. Pt is found within grains and at grain boundaries, where it locally reduces the resistivity, as assessed by in situ four-point-probe electrical conductivity measurement. Our work showcases the correlation between microstructure and electrical conductivity, providing opportunities for future microstructural optimization by tuning the chemical composition at grain boundaries.

cond-mat.mtrl-sci↗

arXiv2021

Investigation of the orientation relationship between nano-sized G-phase precipitates and austenite with scanning nano-beam electron diffraction using a pixelated detector

Scanning nano-beam electron diffraction with a pixelated detector was employed to investigate the orientation relationship of nanometer sized, irradiation induced G-phase (M$_6$Ni$_{16}$Si$_{7}$) precipitates in an austenite matrix. Using this detector, the faint diffraction spots originating from the small G-phase particles could be resolved simultaneously as the intense matrix reflections. The diffraction patterns were analyzed using a two-stage template matching scheme, whereby the matrix is indexed first and the precipitates are indexed second after subtraction of the matrix contribution to the diffraction patterns. The results show that G-phase forms with orientation relationships relative to austenite that are characteristic of face-centered cubic (FCC) to body-centered cubic (BCC) transformations. This work demonstrates that nano-beam electron diffraction with a pixelated detector is a promising technique to investigate orientation relationships of nano-sized precipitates with complex crystal structures in other material systems with relative ease.

cond-mat.mtrl-sci↗

arXiv2021

Dissecting functional degradation in NiTi shape-memory-alloys containing amorphous regions via atomistic simulations

Molecular dynamics simulations are performed to provide a detailed understanding of the functional degradation of shape memory alloys at small scale. The origin of the experimentally reported accumulation of plastic deformation and the anomalous sudden increase of the residual strain under cyclic mechanical loading are explained by detailed insights into the relevant atomic scale processes. Our work reveals that the mechanical response of shape-memory-alloy pillars under cyclic compression is significantly influenced by the presence of an amorphous-like surface region as experimentally induced by focused ion beam milling. The main factor responsible for the observed degradation of superelasticity under cyclic loading is the accumulated plastic deformation and the resultant retained martensite originating from a synergetic contribution of the amorphous and crystalline shape-memory-alloy regions. We show that the reported sudden diminishment of the stress plateaus and hysteresis under cyclic loading is caused by the increased stability of the martensite phase due to the presence of the amorphous phase. Based on the identified mechanism responsible for the degradation, we validate reported methods of recovering the superelasticity and propose a new method to prohibit the synergetic contribution of the amorphous and crystalline regions, such as to achieve a sustainable operation of shape memory alloys at small scale.

cond-mat.mtrl-sci↗

arXiv2021

Automated crystal orientation mapping by precession electron diffraction assisted four-dimensional scanning transmission electron microscopy (4D-STEM) using a scintillator based CMOS detector

The recent development of electron sensitive and pixelated detectors has attracted the use of four-dimensional scanning transmission electron microscopy (4D-STEM). Here, we present a precession electron diffraction assisted 4D-STEM technique for automated orientation mapping using diffraction spot patterns directly captured by an in-column scintillator based complementary metal-oxide-semiconductor (CMOS) detector. We compare the results to a conventional approach, which utilizes a fluorescent screen filmed by an external CCD camera. The high dynamic range and signal-to-noise characteristics of the detector largely improve the image quality of the diffraction patterns, especially the visibility of diffraction spots at high scattering angles. In the orientation maps reconstructed via the template matching process, the CMOS data yields a significant reduction of false indexing and higher reliability compared to the conventional approach. The angular resolution of misorientation measurement could also be improved by masking reflections close to the direct beam. This is because the orientation sensitive, weak and small diffraction spots at high scattering angle are more significant. The results show that fine details such as nanograins, nanotwins and sub-grain boundaries can be resolved with a sub-degree angular resolution which is comparable to orientation mapping using Kikuchi diffraction patterns.

physics.ins-det↗

arXiv2021

Structure and hardness of in situ synthesized nano-oxide strengthened CoCrFeNi high entropy alloy thin films

In this study, we report on face-centered cubic structured CoCrFeNi high-entropy alloy thin films with finely dispersed nano-oxide particles which are formed by internal oxidation. Analytical scanning transmission electron microscopy imaging found that the particles are Cr2O3. The oxide particles contribute to the hardening of the film increasing its hardness by 14% compared to that of the film without precipitates, through the Orowan-type strengthening mechanism. Our novel approach paves the way to design medium- and high-entropy alloys with high strength by making use of oxide phases.

cond-mat.mtrl-sci↗

arXiv2021

Nanocrystalline equiatomic CoCrFeNi alloy thin films: Are they single phase fcc?

The bulk quaternary equiatomic CoCrFeNi alloy is studied extensively in literature. Under experimental conditions, it shows a single-phase fcc structure and its physical and mechanical properties are similar to those of the quinary equiatomic CoCrFeMnNi alloy. Many studies in literature have focused on the mechanical properties of bulk nanocrystalline high entropy alloys or compositionally complex alloys, and their microstructure evolution upon annealing. The thin film processing route offers an excellent alternative to form nanocrystalline alloys. Due to the high nucleation rate and high density of defects in thin films synthesized by sputtering, the kinetics of microstructure evolution is often accelerated compared to those taking place in the bulk. Here, thin films are used to study the phase evolution in nanocrystalline CoCrFeNi deposited on Si/SiO 2 and c-sapphire substrates by magnetron cosputtering from elemental sources. The phases and microstructure of the films are discussed in comparison to the bulk alloy. The main conclusion is that second phases can form even at room temperature provided there are sufficient nucleation sites.

cond-mat.mtrl-sci↗

arXiv2021

Aluminum depletion induced by complex co-segregation of carbon and boron in a Σ 5 [3 1 0] bcc-iron grain boundary

The local variation of grain boundary atomic structure and chemistry caused by segregation of impurities influences the macroscopic properties of poylcrystalline materials. Here, the effect of co-segregation of carbon and boron on the depletion of aluminum at a $Σ5\,(3\,1\,0\,) [0\,0\,1]$ tilt grain boundary in a $α-$Fe-$4~at.~\%$Al bicrystal was studied by combining atomic resolution scanning transmission electron microscopy, atom probe tomography and density functional theory calculations. The atomic grain boundary structural units mostly resemble kite-type motifs and the structure appears disrupted by atomic scale defects. Atom probe tomography reveals that carbon and boron impurities are co-segregating to the grain boundary reaching levels of >1.5 at.\%, whereas aluminum is locally depleted by approx. 2~at.\%. First-principles calculations indicate that carbon and boron exhibit the strongest segregation tendency and their repulsive interaction with aluminum promotes its depletion from the grain boundary. It is also predicted that substitutional segregation of boron atoms may contribute to local distortions of the kite-type structural units. These results suggest that the co-segregation and interaction of interstitial impurities with substitutional solutes strongly influences grain boundary composition and with this the properties of the interface.

cond-mat.mtrl-sci↗

arXiv2020

Strain-Rate-Dependent Deformation Behavior of Ti29Zr24Nb23Hf24 High Entropy Alloys at Elevated and Room Temperature

We investigate the strain-rate-dependent mechanical behavior and deformation mechanisms of a refractory high entropy alloy, Ti29Zr24Nb23Hf24 (at.%), with a single-phase body-centered cubic (BCC) structure. High-temperature compression tests were conducted at temperatures from 700 to 1100°C at strain rates ranging from 10-3 to 10 s-1. A sudden stress drop after yield point was observed at higher temperatures and lower strain rates with the Zener-Holloman parameter, lnZ, in the range of 17.2-20.7. Such a softening behavior can be related to the interaction of dislocations with short-range clustering. However, at higher strain rates or lower temperatures (lnZ>25.0), kink bands were activated being responsible for the continuous strengthening of the alloy in competition with the softening mechanism. Systematic TEM investigations reveal that dislocation walls formed along {110} planes and dislocation loops were observed at a low strain of 6% at a high strain rate of 1 s-1 and 800°C. Kink band induced dynamic recrystallization is evident upon further straining. On the other hand, at low strain rate of 10-3 s-1 and 800°C, discontinuous recrystallization mechanisms become dominant with arrays of dislocations forming in front of the bulged boundaries of parent grains. These sub-grain boundaries eventually turn into high-angle grain boundaries. We also investigate the deformation mechanism of the alloy under extremely high strain rate (103 s-1) at room temperature. The specimen exhibits extensive kink bands with arrays of dislocation walls. As further strained, multiple slip systems can be activated and the interaction of dislocation walls plays a vital role in the strain hardening of the alloy.

cond-mat.mtrl-sci↗

arXiv2020

Faceting diagram for Ag segregation induced nanofaceting at an asymmetric Cu tilt grain boundary

In this work, we experimentally establish the isothermal nanofacet evolution at an asymmetric tilt grain boundary in the Cu-Ag system using a diffusion couple approach. We investigate the nanofacet formation along the grain boundary in dependence of the Ag solute excess concentration. The initial grain boundary dissociates into asymmetric Ag-lean segments and Ag-rich symmetric (210) segments. Increasing Ag excess leads to an increase in Ag-rich facet segment length, while the length of the asymmetric facets remains constant. From this, we construct a grain boundary nanofaceting diagram deduced from our experiments relating local atomic structure, overall inclination and Ag solute excess.

cond-mat.mtrl-sci↗

arXiv2020

Early stage phase separation of AlCoCr0.75Cu0.5FeNi high-entropy powder at the nanoscale

High entropy alloys are generally considered to be single phase material. This state is, however, typically a non-equilibrium state after fabrication at high cooling rates. Phase constitution after fabrication or heat treatment is mostly known for isothermal annealing only and for casts as well as rapidly quenched alloys. Knowledge on early phase separation stages of high entropy alloys and their mechanisms are missing so far. Here, we present results on phase separation at intermediate cooling rates, by characterization of gas atomized powder of the AlCoCr0.75Cu0.5FeNi alloy. Although investigation by X-ray diffraction and Electron Backscatter Diffraction indicates a single-phase nature of the powder particles, aberration-corrected scanning transmission electron microscopy and atom probe tomography reveal a nanoscale phase separation into Ni-Al-rich B2 and Fe-Cr-rich A2 regions as well as a high number density of 3.1x1024 Cu-rich clusters per m3 in the B2 matrix. The observed phase separation and cluster formation are linked to spinodal decomposition and nucleation processes, respectively. The study highlights that adequate characterization techniques need to be chosen when making statements about phase stability and structural evolution in compositionally complex alloys.

cond-mat.mtrl-sci↗

arXiv2020

Microstructure evolution and thermal stability of equiatomic CoCrFeNi films on (0001)alpha-Al2O3

Homogeneous face-centered cubic (fcc) polycrystalline CoCrFeNi films were deposited at room temperature on (0001)alpha-Al2O3 (c-sapphire). Phase and morphological stability of 200 to 670 nm thick films were investigated between 973 K and 1423 K. The fcc-phase persists while the original <111> texture of 30-100 nm wide columnar grains evolves into ~10 or ~1000 micron wide grains. Only the grains having specific orientation relationships to the sapphire grow; as in the case of pure fcc metal (M) films 4 orientation relationships (OR) are found: OR1 (M(111)[1-10]//alpha-Al2O3 (0001)[1-100]) and OR2 (M(111)[1-10]//alpha-Al2O3 (0001)[11-20]) and their twin-related variants (OR1t and OR2t). Below 1000 K, the film microstructure stabilizes into 10 micron wide OR1 and OR1t twin grains independent of film thickness. Above 1000 K, the OR2 and OR2t grains expand to sizes exceeding more than a 1000 times the film thickness. Upon annealing, the films either retain their integrity or break-up depending on the competing kinetics of grain growth and grain boundary grooving. Triple junctions of the grain boundaries, the major actors in film stability, were tracked. Thinner films and higher temperatures favor film break-up by dewetting from the holes grooved at the triple junctions down to the substrate. The grain boundaries of the OR2 and OR2t grains migrate fast enough to overcome the nucleation of holes from which break-up could initiate. The growth of the OR2 and OR2t grains in this complex alloy is faster than in pure fcc metals at equivalent homologous annealing temperatures.

cond-mat.mtrl-sci↗

arXiv2020

Bulk nanostructured AlCoCrFeMnNi chemically complex alloy synthesized by laser-powder bed fusion process

We report the synthesis of a bulk nanostructured alloy using the laser-powder bed fusion process. The equiatomic AlCoCrFeMnNi chemically complex alloy forms a nanoscale modulated structure, which is homogeneously distributed in the as-built condition. The nanostructure consisted of Al & Ni-rich ordered (B2) and Cr & Fe-rich disordered (A2) BCC phases. The two phases form an interconnected phase-network with coherent interface boundaries. Atom-probe-tomography and aberration-corrected scanning transmission electron microscopy analysis of the spatial distribution of the modulated structure suggests the occurrence of nano-scale spinodal decomposition. These results introduce a direct synthesis of bulk nanostructured alloys with promising geometric flexibility.

cond-mat.mtrl-sci↗

arXiv2019

Could face-centered cubic titanium in cold-rolled commercially-pure titanium only be a Ti-hydride?

A face-centered cubic (FCC) phase in electro-polished specimens for transmission electron microscopy of commercially pure titanium has sometimes been reported. Here, a combination of atom-probe tomography, scanning transmission electron microscopy and low-loss electron energy loss spectroscopy is employed to study both the crystal structural and chemical composition of this FCC phase. Our results prove that the FCC phase is actually a TiHx (x>1) hydride, and not a new allotrope of Ti, in agreement with previous reports. The formation of the hydride is discussed.

cond-mat.mtrl-sci↗

arXiv2019

Initiation and stagnation of room temperature grain coarsening in cyclically strained gold films

Despite the large number of experiments demonstrating that grains in a metallic material can grow at room temperature due to applied mechanical load, the mechanisms and the driving forces responsible for mechanically induced grain coarsening are still not understood. Here we present a systematic study of room temperature grain coarsening induced by cyclic strain in thin polymer-supported gold films. By means of detailed electron backscatter diffraction analysis we were able to capture both the growth of individual grains and the evolution of the whole microstructure on the basis of statistical data over thousands of grains. The experimental data are reported for three film thicknesses with slightly different microstructures and three different amplitudes of cyclic mechanical loading. Although different kinds of grain size evolution with increasing cycle number are observed depending on film thickness and strain amplitude, a single model based on a thermodynamic driving force is shown to be capable to explain initiation and stagnation of grain coarsening in all cases. The main implication of the model is that the grains having lower individual yield stress are coarsening preferentially. Besides, it is demonstrated that the existence of local shear stresses imposed on a grain boundary is not a necessary requirement for room-temperature grain coarsening.

cond-mat.mtrl-sci↗

arXiv2018

On the segregation of Re at dislocations in the γ' phase of Ni-based single crystal superalloys

We report evidence of Re and Mo segregation (up to 2.6 at.% and 1 at.%) along with Cr and Co to the dislocations inside of γ' precipitates in a second generation Ni-based single crystal superalloy, after creep deformation at 750°C under an applied stress of 800 MPa. The observed segregation effects can be rationalized through bridging the solute partitioning behavior across the γ/γ' interface and the pipe diffusion mechanism along the core of the dislocation line. This understanding can provide new insights enabling improved alloy design.

cond-mat.mtrl-sci↗